CN112647063A - DLC-nano diamond composite coating preparation method based on laser irradiation - Google Patents
DLC-nano diamond composite coating preparation method based on laser irradiation Download PDFInfo
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- CN112647063A CN112647063A CN202011372926.5A CN202011372926A CN112647063A CN 112647063 A CN112647063 A CN 112647063A CN 202011372926 A CN202011372926 A CN 202011372926A CN 112647063 A CN112647063 A CN 112647063A
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- 239000002113 nanodiamond Substances 0.000 title claims abstract description 115
- 238000000576 coating method Methods 0.000 title claims abstract description 113
- 239000011248 coating agent Substances 0.000 title claims abstract description 112
- 239000002131 composite material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000003746 surface roughness Effects 0.000 claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 claims abstract description 16
- 238000002703 mutagenesis Methods 0.000 claims abstract description 15
- 231100000350 mutagenesis Toxicity 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 238000010329 laser etching Methods 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 32
- 229910003460 diamond Inorganic materials 0.000 claims description 32
- 239000010432 diamond Substances 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002344 surface layer Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 3
- 238000005299 abrasion Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005461 lubrication Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 235000011187 glycerol Nutrition 0.000 description 9
- 238000005498 polishing Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 238000007781 pre-processing Methods 0.000 description 3
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910003481 amorphous carbon Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
- C23C16/27—Diamond only
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- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
- Laser Beam Processing (AREA)
Abstract
A DLC-nano diamond composite coating preparation method based on laser irradiation comprises the following steps: pretreating the surface of the nano diamond coating; focusing a femtosecond laser beam on the top end of the crystal grains on the surface of the pretreated nano-diamond coating, performing femtosecond laser etching scanning treatment, and carrying out in-situ mutagenesis on nano-diamond clusters on the surface of the nano-diamond coating to obtain diamond-like carbon; 3) and carrying out post-treatment on the diamond-like carbon-nano diamond composite coating. The invention not only can prepare the diamond-like film on the surface of the nano diamond coating, but also greatly improves the surface roughness of the diamond-like-nano diamond composite coating, and has obvious gain effect. The surface roughness of the diamond-like carbon-nano diamond composite coating obtained by the invention is greatly reduced, and the friction coefficient of a friction pair and the abrasion loss of a grinding surface can be obviously reduced in the friction process. The preparation method has simple process and low cost, and is very suitable for dry friction and water lubrication working conditions.
Description
Technical Field
The invention relates to a preparation method of a composite coating. In particular to a preparation method of DLC-nano diamond composite coating based on laser irradiation.
Background
The nano diamond coating has excellent mechanical properties and physical properties such as high hardness, high elastic modulus, extremely low friction coefficient, good self-lubricating property, extremely high thermal conductivity and chemical stability, small dielectric constant, wide band gap and the like, and has wide application prospect in the fields of wear-resistant and anti-friction devices and biological implantation devices. However, the surface roughness of the nano-diamond coating prepared by the chemical vapor deposition process is relatively high, and it is not generally directly applicable to the above-mentioned fields. Furthermore, the high surface roughness of the nanodiamond coating tends to result in a relatively high coefficient of friction during rubbing and high wear on the abraded surface.
However, the diamond material has extremely high hardness, the efficiency of the traditional mechanical polishing process is low, curved surfaces are difficult to polish, scratches are easily generated on the surface of the diamond coating, the application of the diamond coating in the field is influenced, and the diamond material is difficult to be directly applied to the precise polishing of the CVD diamond coating. Some researchers have proposed chemical polishing of diamond coatings by utilizing the characteristic that diamond is converted into graphite under certain conditions, but these polishing methods often require the use of special polishing solutions and finally bring about the problem of environmental pollution.
In addition to polishing, the application of solid lubricants to the diamond coated surface is another way to reduce the coefficient of friction of the diamond coating and its amount of wear on the abraded surface. DLC (Diamond-like carbon) film is a film having sp2And sp3The amorphous carbon film has excellent self-lubricating property. The nano-diamond film is simultaneously polished and the diamond-like film is expected to further improve the frictional wear performance of the nano-diamond coating, however, the conventional polishing and diamond-like film preparation composite process is very complicated and has high cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a DLC-nano diamond composite coating preparation method based on laser irradiation, which can greatly improve the surface roughness of the diamond-like carbon-nano diamond composite coating.
The technical scheme adopted by the invention is as follows: a DLC-nano diamond composite coating preparation method based on laser irradiation comprises the following steps:
1) pretreating the surface of the nano diamond coating;
2) focusing a femtosecond laser beam on the top end of the crystal grains on the surface of the pretreated nano-diamond coating, performing femtosecond laser etching scanning treatment, and carrying out in-situ mutagenesis on nano-diamond clusters on the surface of the nano-diamond coating to obtain diamond-like carbon;
3) and carrying out post-treatment on the diamond-like carbon-nano diamond composite coating.
The grain size of the nano diamond coating grains on the surface of the nano diamond coating in the step 1) is 50-100 nm.
The surface roughness of the nano diamond coating in the step 1) is Ra 70-100 nm.
The pretreatment of the step 1) is to immerse the nano diamond coating into a suspension prepared from diamond micro powder and glycerol, perform ultrasonic grinding for 5min, wherein the particle size of the diamond micro powder is 2-5 mu m, then immerse the nano diamond coating into absolute ethyl alcohol, perform ultrasonic cleaning for 5min, and then dry the nano diamond coating.
The ratio of the diamond micro powder to the glycerin in the suspension prepared from the diamond micro powder and the glycerin is 1: 1.
The energy density of the femtosecond laser in the step 2) is 0.34-0.68J/cm2The pulse width was 200fs, the repetition frequency was 50MHz, and the spot diameter was 10 μm.
And 2) the etching scanning interval of the femtosecond laser is 3-5 mu m.
And 3) performing post-treatment, namely placing the diamond-like carbon-nano diamond coating in absolute ethyl alcohol for ultrasonic treatment for 5min, and removing impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after femtosecond laser irradiation.
And 3) after post-treatment, the surface roughness of the finished diamond-like carbon-nano diamond composite coating is Ra 15-30 nm, and the thickness of the surface diamond-like carbon film is 50-100 nm.
The method for preparing the DLC-nano diamond composite coating based on laser irradiation not only can prepare the diamond-like film on the surface of the nano diamond coating, but also greatly improves the surface roughness of the diamond-like film-nano diamond composite coating, and has obvious gain effect. According to the invention, a femtosecond laser irradiation method is adopted to induce the diamond component on the surface layer of the nano-diamond coating into the diamond-like component in situ, so that the surface roughness of the obtained diamond-like-nano-diamond composite coating is greatly reduced compared with the nano-diamond coating which is not subjected to femtosecond laser irradiation, and the friction coefficient of a friction pair and the abrasion loss to a grinding surface can be obviously reduced in the friction process. The preparation method has simple process and low cost, and is very suitable for dry friction and water lubrication working conditions.
Drawings
FIG. 1 is a polishing flow chart of the laser irradiation-based DLC-nanodiamond composite coating preparation method of the present invention;
fig. 2 is an SEM picture of the surface topography of an example prepared diamond-like-nanodiamond composite coating;
figure 3 is an SEM picture of the cross-sectional morphology of the diamond-like-nanodiamond composite coating prepared in example 1;
FIG. 4 is an XPS spectrum of a diamond-like-nanodiamond composite coating prepared in example 1;
figure 5 is an SEM picture of the surface topography of the diamond-like-nanodiamond composite coating prepared in example 2;
figure 6 is an SEM picture of the cross-sectional morphology of the diamond-like-nanodiamond composite coating prepared in example 2.
Detailed Description
The method for preparing DLC-nanodiamond composite coating layer based on laser irradiation according to the present invention will be described in detail with reference to the following examples and accompanying drawings.
As shown in FIG. 1, the preparation method of the DLC-nanodiamond composite coating based on laser irradiation comprises the following steps:
1) pretreating the surface of the nano diamond coating; wherein the content of the first and second substances,
the grain size of the nano diamond coating grains on the surface of the nano diamond coating is 50-100 nm. The surface roughness of the nano diamond coating is Ra 70-100 nm.
And the pretreatment comprises the steps of immersing the nano diamond coating into turbid liquid prepared from diamond micro powder and glycerol, carrying out ultrasonic grinding for 5min, immersing the diamond micro powder with the particle size of 2-5 mu m into absolute ethyl alcohol, carrying out ultrasonic cleaning for 5min, and drying. The ratio of the diamond micro powder to the glycerin in the suspension prepared from the diamond micro powder and the glycerin is 1: 1.
2) Focusing a femtosecond laser beam on the top end of the crystal grain on the surface of the pretreated nano-diamond coating, performing femtosecond laser etching scanning treatment, and carrying out in-situ mutagenesis on the nano-diamond cluster on the surface of the nano-diamond coating to obtain diamond-like carbon (DLC); wherein the content of the first and second substances,
the energy density of the femtosecond laser is 0.34-0.68J/cm2The pulse width was 200fs, the repetition frequency was 50MHz, and the spot diameter was 10 μm. The etching scanning interval of the femtosecond laser is 3-5 mu m.
3) Carrying out post-treatment on the diamond-like carbon-nano diamond composite coating; wherein the content of the first and second substances,
the post-treatment is to place the diamond-like carbon-nano diamond coating in absolute ethyl alcohol for ultrasonic treatment for 5min to remove impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after femtosecond laser irradiation.
After post-treatment, the surface roughness of the finished diamond-like carbon-nano diamond composite coating is Ra 15-30 nm, and the thickness of the diamond-like carbon film on the surface layer is 50-100 nm.
The method for preparing the laser irradiation-based DLC-nanodiamond composite coating according to the present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1:
the nano diamond coating with the grain size of 50nm and the surface roughness Ra 70nm is taken as an object to carry out femtosecond laser irradiation. Firstly, preprocessing the surface of a nano diamond coating, immersing the nano diamond coating into turbid liquid prepared from diamond micro powder and glycerol, carrying out ultrasonic grinding for 5min, wherein the particle size of the diamond micro powder is 2 mu m, then immersing the nano diamond coating into absolute ethyl alcohol, carrying out ultrasonic cleaning for 5min, and then drying.
The pulse width is 200fs, and the energy density is 0.34J/cm2And the femtosecond laser with the repetition frequency of 50MHz and the spot diameter of 10 μm focuses the femtosecond laser beam on the surface of the micron diamond coating, and performs femtosecond laser irradiation scanning treatment with the scanning interval of 3 μm. And (3) carrying out in-situ mutagenesis on the nano-diamond component on the nano-diamond surface layer into the diamond-like component by femtosecond laser irradiation.
And (3) placing the diamond-like carbon-nano diamond composite coating in absolute ethyl alcohol for ultrasonic treatment for 5min, and removing impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after femtosecond laser irradiation.
The thickness of the diamond-like carbon film on the surface layer of the prepared diamond-like carbon-nano diamond composite coating is 50nm, and the surface roughness is reduced from Ra 70nm to 30 nm.
Fig. 2 is an SEM picture of the surface topography of the diamond-like-nano diamond composite coating prepared in this example. Fig. 3 is an SEM picture of the cross-sectional morphology of the diamond-like-nano diamond composite coating prepared in this example. Fig. 4 is an XPS spectrum of the diamond-like-nanodiamond composite coating prepared in this example.
Example 2:
the nano diamond coating with the grain size of 100nm and the surface roughness Ra 100nm is taken as an object to carry out femtosecond laser irradiation. Firstly, preprocessing the surface of a nano diamond coating, immersing the nano diamond coating into turbid liquid prepared from diamond micro powder and glycerol, carrying out ultrasonic grinding for 5min, wherein the particle size of the diamond micro powder is 5 mu m, then immersing the nano diamond coating into absolute ethyl alcohol, carrying out ultrasonic cleaning for 5min, and then drying.
The pulse width is 200fs, and the energy density is 0.68J/cm2A femtosecond laser with repetition frequency of 50MHz and spot diameter of 10 μmThe femtosecond laser beam is focused on the surface of the micron diamond coating, and the femtosecond laser irradiation scanning treatment is carried out, wherein the scanning distance is 5 mu m. And (3) carrying out in-situ mutagenesis on the nano-diamond component on the nano-diamond surface layer into the diamond-like component by femtosecond laser irradiation.
And (3) placing the diamond-like carbon-nano diamond composite coating in absolute ethyl alcohol for ultrasonic treatment for 5min, and removing impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after femtosecond laser irradiation.
The thickness of the diamond-like film on the surface layer of the prepared diamond-like-nano diamond composite coating is 100nm, and the surface roughness is reduced from Ra 100nm to 15 nm.
Fig. 5 is an SEM picture of the surface topography of the diamond-like-nanodiamond composite coating prepared in this example. Fig. 6 is an SEM picture of the cross-sectional morphology of the diamond-like-nano diamond composite coating prepared in this example.
Example 3:
the nano diamond coating with the grain size of 50nm and the surface roughness Ra 80nm is taken as an object to carry out femtosecond laser irradiation. Firstly, preprocessing the surface of a nano diamond coating, immersing the nano diamond coating into turbid liquid prepared from diamond micro powder and glycerol, carrying out ultrasonic grinding for 5min, wherein the particle size of the diamond micro powder is 3.5 mu m, then immersing the nano diamond coating into absolute ethyl alcohol, carrying out ultrasonic cleaning for 5min, and then drying.
The pulse width is 200fs, and the energy density is 0.5J/cm2And the femtosecond laser with the repetition frequency of 50MHz and the spot diameter of 10 μm focuses the femtosecond laser beam on the surface of the micron diamond coating, and performs femtosecond laser irradiation scanning treatment with the scanning interval of 4 μm. And (3) carrying out in-situ mutagenesis on the nano-diamond component on the nano-diamond surface layer into the diamond-like component by femtosecond laser irradiation.
And (3) placing the diamond-like carbon-nano diamond composite coating in absolute ethyl alcohol for ultrasonic treatment for 5min, and removing impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after femtosecond laser irradiation.
The thickness of the diamond-like film on the surface layer of the prepared diamond-like-nano diamond composite coating is 100nm, and the surface roughness is reduced from Ra 80nm to 30 nm.
Claims (9)
1. A DLC-nano diamond composite coating preparation method based on laser irradiation is characterized by comprising the following steps:
1) pretreating the surface of the nano diamond coating;
2) focusing a femtosecond laser beam on the top end of the crystal grains on the surface of the pretreated nano-diamond coating, performing femtosecond laser etching scanning treatment, and carrying out in-situ mutagenesis on nano-diamond clusters on the surface of the nano-diamond coating to obtain diamond-like carbon;
3) and carrying out post-treatment on the diamond-like carbon-nano diamond composite coating.
2. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein the grain diameter of the nano diamond coating crystal grains on the surface of the nano diamond coating in the step 1) is 50-100 nm.
3. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein the surface roughness of the nano diamond coating in the step 1) is Ra 70-100 nm.
4. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to the claim 1, characterized in that the pretreatment of the step 1) is to immerse the nano diamond coating into a suspension prepared by diamond micro powder and glycerol for ultrasonic grinding for 5min, wherein the grain diameter of the diamond micro powder is 2-5 μm, then immerse the nano diamond coating into absolute ethyl alcohol for ultrasonic cleaning for 5min, and then dry the diamond coating.
5. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis as claimed in claim 4, wherein the ratio of the diamond micro powder to the glycerol in the suspension prepared from the diamond micro powder and the glycerol is 1: 1.
6. The method for preparing the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein the energy density of the femtosecond laser in the step 2) is 0.34-0.68J/cm2The pulse width was 200fs, the repetition frequency was 50MHz, and the spot diameter was 10 μm.
7. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein the etching scanning interval of the femtosecond laser in the step 2) is 3-5 μm.
8. The method for preparing a diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein the post-treatment in the step 3) is to place the diamond-like carbon-nano diamond coating in absolute ethyl alcohol for ultrasonic treatment for 5min to remove impurities remained on the surface of the diamond-like carbon-nano diamond composite coating after the femtosecond laser irradiation.
9. The preparation method of the diamond-like carbon-nano diamond composite coating based on femtosecond laser irradiation in-situ mutagenesis according to claim 1, wherein after the post-treatment in the step 3), the surface roughness of the finished diamond-like carbon-nano diamond composite coating is Ra 15-30 nm, and the thickness of the diamond-like carbon film on the surface layer is 50-100 nm.
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Cited By (4)
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| CN113681168A (en) * | 2021-09-10 | 2021-11-23 | 郑州磨料磨具磨削研究所有限公司 | Method for uniformly processing diamond film surface by using pulsed laser ablation |
| CN113832447A (en) * | 2021-09-08 | 2021-12-24 | 宁波杭州湾新材料研究院 | Conductive self-lubricating composite coating and preparation method thereof |
| CN116247017A (en) * | 2023-02-06 | 2023-06-09 | 中国人民解放军国防科技大学 | Diamond substrate sp 3 -sp 2 Preparation method and application of hybrid bond network layer |
| CN113832447B (en) * | 2021-09-08 | 2024-05-31 | 宁波杭州湾新材料研究院 | Conductive self-lubricating composite coating and preparation method thereof |
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| CN112647063B (en) | 2022-06-07 |
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